Sodium Hydroxide → HCID 20130662、化合物

HRID 1252940ノート

反応式

HRID 1252940 の反応式
[Cl:1][C:2]1[CH:12]=[CH:11][C:10]([N:13]2[C:22](=[O:23])[C:21]3[CH2:20][CH2:19][CH2:18][CH2:17][C:16]=3[N:15]([CH3:24])[C:14]2=[O:25])=[CH:9][C:3]=1[C:4]([O:6]CC)=[O:5].[OH-].[Na+]>C(O)C.O>[Cl:1][C:2]1[CH:12]=[CH:11][C:10]([N:13]2[C:22](=[O:23])[C:21]3[CH2:20][CH2:19][CH2:18][CH2:17][C:16]=3[N:15]([CH3:24])[C:14]2=[O:25])=[CH:9][C:3]=1[C:4]([OH:6])=[O:5]

参加物

5

実験手順

A solution of 3.6 g of ethyl 2-chloro-5-[1,4,5,6,7,8-hexahydro-1-methyl-2,4-dioxo-3-(2H)-quinazolinyl]-benzoate in 70 ml of ethanol is held at 60° C. for 10 minutes with 0.6 g of sodium hydroxide in 70 ml of water and subsequently stirred for 1 hour. The solution is substantially evaporated down under reduced pressure and the residue is brought to pH 1 with 2N hydrochloric acid. The precipitate is shaken five times with 50 ml amounts of diethyl ether and the organic phases are dried over anhydrous sodium sulphate and evaporated to dryness under reduced pressure. 2-Chloro-5-[1,4,5,6,7,8-hexahydro-1-methyl-2,4-dioxo-3-(2H)-quinazolinyl]-benzoic acid is obtained.

後処理

  1. customThe solution is substantially evaporated down under reduced pressure
  2. stirringThe precipitate is shaken five times with 50 ml amounts of diethyl ether
  3. dry with materialthe organic phases are dried over anhydrous sodium sulphate
  4. customevaporated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-b29dbd605cd14ddabfb1064976227c6c
出典データセット
uspto-grants-1988_05
特許番号
US04746352

反応ノート

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